CN103074619A - Graphene oxide-silver compound particle and preparation method thereof - Google Patents
Graphene oxide-silver compound particle and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a graphene oxide-silver compound particle and a preparation method thereof. The graphene oxide and silver compound particle is in a core-shell structure; a core is an organic matter or inorganic matter particle; and a shell is the graphene oxide-silver compound particle. The preparation method particularly comprises the following steps of: preparing a water solution containing graphene oxide; preparing a suspension solution of the organic matter or inorganic matter particle; preparing the core-shell structure compound particle covered by graphene oxide on the surface; mixing the core-shell structure compound particle covered by graphene oxide on the surface with a silver nitrate solution; adding a reducing agent to carry out one-step reduction reaction under a nitrogen atmosphere; and naturally cooling a reaction solution to a room temperature, centrifuging, washing and drying to obtain the graphene oxide-silver compound particle. According to the graphene oxide-silver compound particle and the preparation method thereof disclosed by the invention, the performance of the finally-obtained graphene oxide-silver compound particle is very good, the utilization amount of the reducing agent used in a preparation process is less and the production cost is low.
Description
Technical field
The present invention relates to a kind of graphene oxide-Yin composite particles and preparation method thereof.
Background technology
Graphene is a kind of novel Two-dimensional Carbon material, because its unique structure makes it have the performance of special electricity, mechanics and chemical aspect, therefore in fields such as catalysis, sensor, microelectronics huge application potential is arranged, be subject to investigator's extensive concern.
Therefore Nano silver grain and matrix material thereof have special electronic structure, have important using value in sensing, surface enhanced Raman scattering, biomarker and the aspect such as antibiotic.The graphene-silver nano particle mixture, owing to wherein there being stronger interaction between Graphene and the Nano silver grain, verified its has than independent Graphene or more excellent optics, photochemical catalysis and the surface-enhanced Raman performance of Nano silver grain.[Mingshan?Zhu,?Penglei?Chen,?and?Minghua?Liu,?ACS?Nano,?5(?6),?2011,?4529–4536]
The defectives such as the method for preparing Graphene reduction-oxidation graphite commonly used at present when the standby graphene oxide of reduction-oxidation graphite-made, exists the recovery time long, and the reductive agent consumption is large.In addition, the graphene oxide that reduction obtains regenerates graphite because its hydrophobic characteristic under Van der Waals force and π-π interaction, is easy to occur irreversible reunion, has a strong impact on the performance of Graphene performance.And, if do not add any processing, directly silver being incorporated in the graphene oxide, the dispersion situation of Nano silver grain in Graphene is undesirable, and this also can directly have influence on the performance of argent.
Summary of the invention
One of purpose of the present invention is to provide a kind of graphene oxide and silver-colored composite particles in order to solve above-mentioned technical problem.
A kind of graphene oxide that two of purpose of the present invention is to provide above-mentioned and the preparation method of silver-colored composite particles.The method is namely utilized the principle of self-assembly, graphite oxide and silver ions successively are assembled into the surface of organism particle or inorganic particles, then by a stage reduction method graphite oxide and silver ions are reduced simultaneously, finally obtain a kind of graphene oxide and silver-colored composite particles, this graphene oxide and silver-colored composite particles have nucleocapsid structure.
Technical scheme of the present invention
A kind of graphene oxide and silver-colored composite particles, be nucleocapsid structure, its nuclear is organism particle or inorganic particles, shell is graphene oxide-Nano silver grain, wherein organism particle or inorganic particles and graphene oxide-Nano silver grain calculate in mass ratio, i.e. organism particle or inorganic particles: graphene oxide: Nano silver grain is 100:1-2:0.5-1.
Above-mentioned organism particle is about to polymerization single polymerization monomer and obtains by methods such as letex polymerization, suspension polymerization or dispersion polymerizations; Described polymerization single polymerization monomer is methyl methacrylate, β-dimethyl-aminoethylmethacrylate, first class butyl acrylate, Rocryl 410, methyl acrylate, ethyl propenoate, butyl acrylate, the mixture of one or more compositions in Hydroxyethyl acrylate and the vinylbenzene;
Above-mentioned inorganic particles is silicon dioxide granule, calcium carbonate particles, TiO 2 particles, Z 250 particle or aluminium oxide particles etc.
Above-mentioned a kind of graphene oxide and the preparation method of silver-colored composite particles specifically comprise the steps:
(1), the preparation of the aqueous solution of graphite oxide
In deionized water, the concentration of graphite oxide is 0.5-5mg/mL with the graphite oxide ultra-sonic dispersion;
(2), the preparation of the suspension of organism particle or inorganic particles
Organism particle or inorganic particles are dispersed in the deionized water, dispersed with stirring obtains the suspension of organism particle or inorganic particles, to by letex polymerization, dispersion polymerization or suspension polymerization obtain the polymer particle aqueous dispersion, can directly be diluted to desired concn and get final product;
(3), the organism particle of step (2) gained or the suspension of inorganic particles are joined in the graphite oxide aqueous solution of step (1) gained, leave standstill for some time after centrifugation obtain the nucleocapsid structure composite particles that the surface coats graphite oxide;
(4), the nucleocapsid structure composite particles that the surface that step (3) is obtained coats graphite oxide mixes with silver nitrate solution, add reductive agent, then under nitrogen atmosphere, solution temperature is raised to 70-90 ℃ and carries out reduction reaction 5-7h, the reaction solution of gained naturally cools to room temperature, centrifugal, the solid that obtains is 40-60 ℃ and carries out drying through deionized water wash, control temperature, namely obtain graphene oxide-Yin composite particles;
Described reductive agent is sodium borohydride, hydrazine hydrate, lithium aluminum hydride, ethanol or ethylene glycol etc., be preferably sodium borohydride or hydrazine hydrate, described reductive agent consumption calculates by itself and the mass ratio that finally obtains organism particle in graphene oxide-Yin composite particles or inorganic particles, graphene oxide-Nano silver grain, i.e. organism particle or inorganic particles: graphene oxide: Nano silver grain: reductive agent is 100:1-2:0.8-1.6:0.08.
Beneficial effect of the present invention
The preparation method of a kind of graphene oxide of the present invention and silver-colored composite particles, owing in the preparation process graphite oxide is wrapped in inorganic particles or organism particle surface, therefore in the process of reduction preparation graphene oxide, avoid the reunion of Graphene, be conducive to the performance of Graphene performance.
The preparation method of a kind of graphene oxide of the present invention and silver-colored composite particles, because graphene oxide and Nano silver grain are evenly distributed on the surface of organism particle or inorganic particles, thereby be conducive to synergistic performance between graphene oxide-Nano silver grain, improve the performance of graphene oxide-Nano silver grain.
The preparation method of a kind of graphene oxide of the present invention and silver-colored composite particles, because graphene oxide and silver are the surfaces that is wrapped in organism particle or inorganic particles, the to a certain extent greatly reduction of accelerating oxidation graphite of existence of silver, therefore only need relatively less reductive agent just can obtain the graphene oxide of identical reducing degree, reduce the consumption of reductive agent, thereby reduced the production cost of graphene oxide and silver-colored composite particles.
Description of drawings
The graphene oxide of Fig. 1, embodiment 1 gained and silver-colored composite particles are dispersed in the transmission electron microscope picture on the copper mesh, acceleration voltage 200kV, and magnification * 75000;
The graphene oxide of Fig. 2, embodiment 1 gained and silver-colored composite particles are dispersed in the transmission electron microscope picture on the copper mesh, acceleration voltage 200kV, and magnification * 30000;
The graphene oxide of Fig. 3, embodiment 1 gained and the scanning electron microscope (SEM) photograph of silver-colored composite particles.
Embodiment;
Also by reference to the accompanying drawings the present invention is further set forth below by specific embodiment, but do not limit the present invention.
Various raw material informations used in the various embodiments of the present invention are as follows:
5% (w/v) polystyrene microsphere aqueous solution is purchased from Zhejiang permanent brightness chemical industry company limited; Graphite Powder 99 (mean sizes 30 μ m, purity〉95%) and other reagent (being analytical pure) are purchased from Solution on Chemical Reagents in Shanghai company limited.
Analyze used instrument information in the embodiment of the invention as follows:
JEM1400 transmission electron microscope (Japan) and FEI NOVA NanoSEM 450 (U.S.) scanning electron microscope.
Embodiment 1
A kind of graphene oxide and silver-colored composite particles, be nucleocapsid structure, its nuclear is the organism particle, shell is graphene oxide-Nano silver grain, wherein organism particle and graphene oxide-Nano silver grain calculate in mass ratio, i.e. the organism particle: graphene oxide: Nano silver grain is 100:1:0.5;
Described organism particle is polystyrene microsphere.
Above-mentioned a kind of graphene oxide and the preparation method of silver-colored composite particles specifically comprise the steps:
(1), concentration is 1mgmL
-1The preparation of the graphite oxide aqueous solution
Taking by weighing 50mg joins in the 20mL deionized water by the standby graphite oxide (ACS Nano 4 (2010) 6697 for A. Wojcik, P. V. Kamat) of Hummers legal system, ultra-sonic dispersion is even, be transferred in the 50mL volumetric flask constant volume, first ultrasonic 1h all before follow-up each use;
(2), the preparation of the suspension of organism particle
The suspension of the organism particle that the present embodiment is used is that concentration is the 50mg/mL polystyrene microsphere aqueous solution, directly buys in Zhejiang perseverance brightness chemical industry company limited;
(3), be that the concentration that the 50mg/mL polystyrene microsphere aqueous solution joins 2.5mL step (1) gained is 1mgmL with 5mL concentration
-1In the graphite oxide aqueous solution, at room temperature stir and spend the night, centrifugal, deionized water wash, the solid that obtains are the nucleocapsid structure composite particles that the surface coats graphite oxide;
It is 1mgmL that the nucleocapsid structure composite particles of the surface coating graphite oxide that (4), step (3) is obtained is distributed to 2mL concentration
-1Silver nitrate aqueous solution in, continue to stir 4h after, adding 2mL concentration is 0.1molL
-1The borane reducing agent sodium hydride aqueous solution, then under nitrogen atmosphere, be heated to 90 ℃, and carry out reduction reaction 5h under stirring, the reaction solution of gained naturally cools to after the room temperature centrifugal, the solid substance that obtains is controlled temperature be 40-60 ℃ and carry out drying behind deionized water wash, namely obtain the graphene oxide with nucleocapsid structure and the silver-colored composite particles of favorable dispersity.
The graphene oxide of above-mentioned gained and silver-colored composite particles carry out transmission electron microscope observing through being dispersed on the copper mesh, at acceleration voltage 200kV, the result who observes under the condition of magnification * 75000 as shown in Figure 1, as can be seen from Figure 1, it has nucleocapsid structure.
Further, at acceleration voltage 200kV, magnification * 30000 proceeds to observe to above-mentioned graphene oxide and the silver-colored composite particles that is dispersed on the copper mesh by transmission electron microscope, its result as shown in Figure 2, graphene oxide/Nano silver grain is evenly distributed on the surface of organism particle polystyrene microsphere nuclear structure as shell as can be drawn from Figure 2.
In addition, by scanning electron microscope graphene oxide and the silver-colored composite particles of above-mentioned gained carried out scanning analysis, the result as shown in Figure 3, as can be seen from Figure 3 in the graphene oxide of above-mentioned gained and the silver-colored composite particles, the favorable dispersity of graphene oxide and Nano silver grain.
Embodiment 2
A kind of graphene oxide and silver-colored composite particles, be nucleocapsid structure, its nuclear is the organism particle, shell is graphene oxide-Nano silver grain, wherein organism particle and graphene oxide-Nano silver grain calculate in mass ratio, i.e. the organism particle: graphene oxide: Nano silver grain is 100:2:0.5;
Described organism particle is polystyrene microsphere.
Above-mentioned a kind of graphene oxide and the preparation method of silver-colored composite particles specifically comprise the steps:
(1), concentration is 1mgmL
-1The preparation of the graphite oxide aqueous solution
With embodiment 1;
(2), the preparation of the suspension of organism particle
The suspension of the organism particle that the present embodiment is used is that concentration is the 50mg/mL polystyrene microsphere aqueous solution, directly buys in Zhejiang perseverance brightness chemical industry company limited;
(3), with 5mL concentration be the 1mgmL that the 50mg/mL polystyrene microsphere aqueous solution joins 5mL step (1) gained
-1In the graphite oxide aqueous solution, at room temperature stir and spend the night, centrifugal, deionized water wash, the solid that obtains are the nucleocapsid structure composite particles that the surface coats graphite oxide;
It is 1 mgmL that the nucleocapsid structure composite particles of the surface coating graphite oxide that (4), step (3) is obtained is distributed to 2mL concentration
-1Silver nitrate aqueous solution in, continue to stir 4h after, adding 2mL concentration is 0.1 molL
-1The borane reducing agent sodium hydride aqueous solution, then under nitrogen atmosphere, be heated to 90 ℃, and carry out reduction reaction 5h under stirring, the reaction solution of gained naturally cools to after the room temperature centrifugal, the solid substance that obtains is controlled temperature be 40-60 ℃ and carry out drying behind deionized water wash, namely obtain the graphene oxide with nucleocapsid structure and the silver-colored composite particles of favorable dispersity.
Embodiment 3
A kind of graphene oxide and silver-colored composite particles, be nucleocapsid structure, its nuclear is the organism particle, shell is graphene oxide-Nano silver grain, wherein organism particle and graphene oxide-Nano silver grain calculate in mass ratio, i.e. the organism particle: graphene oxide: Nano silver grain is 100:1.5:0.5;
Described organism particle is polystyrene microsphere.
Above-mentioned a kind of graphene oxide and the preparation method of silver-colored composite particles specifically comprise the steps:
(1), concentration is 1mgmL
-1The preparation of the graphite oxide aqueous solution
With embodiment 1;
(2), the preparation of the suspension of organism particle
The suspension of the organism particle that the present embodiment is used is that concentration is the 50mg/mL polystyrene microsphere aqueous solution, directly buys in Zhejiang perseverance brightness chemical industry company limited;
(3), be that the concentration that the 50mg/mL polystyrene microsphere aqueous solution joins 3.75mL step (1) gained is 1mgmL with 5mL concentration
-1In the graphite oxide aqueous solution, at room temperature stirring is spent the night, centrifugal, deionized water wash, and the solid that obtains is the nucleocapsid structure composite particles that the surface coats graphite oxide;
It is 1mgmL that the nucleocapsid structure composite particles of the surface coating graphite oxide that (4), step (3) is obtained is distributed to 2mL concentration
-1Silver nitrate aqueous solution in, continue to stir 4h after, adding 2mL concentration is 0.1molL
-1The borane reducing agent sodium hydride aqueous solution, then under nitrogen atmosphere, be heated to 90 ℃, and carry out reduction reaction 5h under stirring, the reaction solution of gained naturally cools to after the room temperature centrifugal, the solid substance that obtains is controlled temperature be 40-60 ℃ and carry out drying behind deionized water wash, namely obtain the graphene oxide with nucleocapsid structure and the silver-colored composite particles of favorable dispersity.
Embodiment 4
A kind of graphene oxide and silver-colored composite particles, be nucleocapsid structure, its nuclear is the organism particle, and shell is graphene oxide-Nano silver grain, wherein organism particle and graphene oxide-Nano silver grain calculate in mass ratio, i.e. the organism particle: graphene oxide: Nano silver grain is 100:2:1;
Described organism particle is polystyrene microsphere.
Above-mentioned a kind of graphene oxide and the preparation method of silver-colored composite particles specifically comprise the steps:
(1), concentration is 1mgmL
-1The preparation of the graphite oxide aqueous solution
With embodiment 1;
(2), the preparation of the suspension of organism particle
The suspension of the organism particle that the present embodiment is used is that concentration is the 50mg/mL polystyrene microsphere aqueous solution, directly buys in Zhejiang perseverance brightness chemical industry company limited;
(3), be that the concentration that the 50mg/mL polystyrene microsphere aqueous solution joins 5mL step (1) gained is 1mgmL with 5mL concentration
-1In the graphite oxide aqueous solution, at room temperature stir and spend the night, centrifugal, deionized water wash, the solid that obtains are the nucleocapsid structure composite particles that the surface coats graphite oxide;
It is 1.0mgmL that the nucleocapsid structure composite particles of the surface coating graphite oxide that (4), step (3) is obtained is distributed to 4mL concentration
-1Silver nitrate aqueous solution in, continue to stir 4h after, adding 2mL concentration is 0.1molL
-1The reductive agent hydrazine hydrate aqueous solution, then under nitrogen atmosphere, be heated to 90 ℃, and carry out reduction reaction 5h under stirring, the reaction solution of gained naturally cools to after the room temperature centrifugal, the solid substance that obtains is controlled temperature be 40-60 ℃ and carry out drying behind deionized water wash, namely obtain the graphene oxide with nucleocapsid structure and the silver-colored composite particles of favorable dispersity.
Foregoing only is the basic explanation of the present invention under conceiving, and according to any equivalent transformation that technical scheme of the present invention is done, all should belong to protection scope of the present invention.
Claims (6)
1. a graphene oxide and silver-colored composite particles, it is characterized in that described graphene oxide and silver-colored composite particles are nucleocapsid structure, described nuclear is organism particle or inorganic particles, described shell is graphene oxide-Nano silver grain, wherein organism particle or inorganic particles and graphene oxide-Nano silver grain calculate in mass ratio, i.e. organism particle or inorganic particles: graphene oxide: Nano silver grain is 100:1-2:0.8-1.6.
2. a kind of graphene oxide as claimed in claim 1 and silver-colored composite particles is characterized in that described organism particle is about to polymerization single polymerization monomer and obtains by letex polymerization, suspension polymerization or dispersion polymerization processes;
Described polymerization single polymerization monomer is methyl methacrylate, β-dimethyl-aminoethylmethacrylate, first class butyl acrylate, Rocryl 410, methyl acrylate, ethyl propenoate, butyl acrylate, the mixture of one or more compositions in Hydroxyethyl acrylate and the vinylbenzene;
Described inorganic particles is silicon dioxide granule, calcium carbonate particles, TiO 2 particles, Z 250 particle or aluminium oxide particles.
3. the preparation method of a kind of graphene oxide as claimed in claim 1 or 2 and silver-colored composite particles is characterized in that specifically comprising the steps:
(1), the preparation of the aqueous solution of graphite oxide
In deionized water, the concentration of graphite oxide is 0.5-5mg/mL with the graphite oxide ultra-sonic dispersion;
(2), the preparation of the suspension of organism particle or inorganic particles
Organism particle or inorganic particles are dispersed in the deionized water, and dispersed with stirring obtains the suspension of organism particle or inorganic particles;
(3), the organism particle of step (2) gained or the suspension of inorganic particles are joined in the graphite oxide aqueous solution of step (1) gained, leave standstill rear centrifugation and obtain the nucleocapsid structure composite particles that the surface coats graphite oxide;
(4), the nucleocapsid structure composite particles that the surface that step (3) is obtained coats graphite oxide mixes with silver nitrate solution, add reductive agent, then under nitrogen atmosphere, solution temperature is raised to 70-90 ℃ and carries out reduction reaction 5-7h, the reaction solution of gained naturally cools to room temperature, centrifugal, the solid that obtains is 40-60 ℃ and carries out drying through deionized water wash, control temperature, namely obtain the graphene oxide of nucleocapsid structure-Yin composite particles.
4. the preparation method of a kind of graphene oxide as claimed in claim 3 and silver-colored composite particles is characterized in that the reductive agent described in the step (4) is sodium borohydride, hydrazine hydrate, lithium aluminum hydride, ethanol or ethylene glycol.
5. the preparation method of a kind of graphene oxide as claimed in claim 4 and silver-colored composite particles, it is characterized in that the reductive agent consumption described in the step (4) by its with final resulting graphene oxide-Yin composite particles in organism particle or the mass ratio calculating of inorganic particles, graphene oxide-Nano silver grain, i.e. organism particle or inorganic particles: graphene oxide: Nano silver grain: reductive agent is 100:1-2:0.8-1.6:0.08.
6. the preparation method of a kind of graphene oxide as claimed in claim 5 and silver-colored composite particles, the concentration that it is characterized in that the aqueous solution of the graphite oxide described in the step (1) is 1mg/mL, the suspension of the organism particle described in the step (2) is that concentration is the 50mg/mL polystyrene microsphere aqueous solution, and the used silver nitrate aqueous solution concentration of step (4) is 1.0mgmL
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